m-Chloroperbenzoic acid → HCID 21283336, Verbindung

HRID 2232233Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2232233
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]3=[N:30][N:31]=[C:32]([S:33][CH3:34])[N:22]3[N:21]=2)=[CH:16][CH:15]=1>C(Cl)Cl>[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]3=[N:30][N:31]=[C:32]([S:33]([CH3:34])=[O:9])[N:22]3[N:21]=2)=[CH:16][CH:15]=1

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 21283334HCID 21283334, Verbindung

Produkt 1

HCID 21283336HCID 21283336, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

3-Chloroperbenzoic acid (2.2 g) is added to a solution of 6-(4-methoxyphenyl)-3-(methylthio)-1,2,4-triazolo[3,4-a]phthalazine (4 g) in methylene chloride (120 ml) and the obtained mixture is stirred at room temperature for 5 hours. The solution is washed with sodium metabisulfite first and then with sodium bicarbonate. The organic solution is then dried over MgSO4 and concentrated to dryness by evaporating off the solvent. The residue thus obtained is crystallized from ethanol yielding 4 g of the compound of the title. M.p. 201°-03° C.

Aufarbeitung

  1. washThe solution is washed with sodium metabisulfite first
  2. dry with materialThe organic solution is then dried over MgSO4
  3. concentrationconcentrated to dryness
  4. customby evaporating off the solvent
  5. customThe residue thus obtained
  6. customis crystallized from ethanol yielding 4 g of the compound of the title

Quellen und Nachweise

ORD-Eintrag
ord-350290d39b944b0786a02776330d47bd
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04788186

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